Analyzing Li-NMC cathodes and battery material precursors: Why XRF with tailored CRMs is the optimal solution

X-ray fluorescence (XRF) spectrometry is a fast, routine way to measure the elemental make-up of lithium nickel manganese cobalt oxide (Li-NMC) cathodes.

On its own, though, standard XRF is only semi-quantitative: production-grade accuracy depends on calibrating against appropriate reference materials. For battery materials, these have traditionally been scarce. We set out to close that gap.

Here’s how the Revontium energy-dispersive XRF spectrometer, in conjunction with calibration against our NMC-specific certified reference materials (CRMs), delivers fully quantitative, validated results.

Why elemental analysis matters for NMC cathodes

The proportions of Ni, Mn, and Co drive cathode performance: energy density, stability, safety, and lifetime. That makes accurate elemental analysis essential across raw-material qualification, process control, R&D, and quality assurance.

Why you need NMC-specific CRMs

XRF is only as good as the materials used to calibrate it. Your CRMs can be the difference between a rough screen and a production-grade measurement of your cathode and precursor materials – but battery-material standards are scarce.

To close that gap, Malvern Panalytical has developed 12 synthetic NMC CRMs specifically for XRF calibration using fused beads.

The outcome: XRF results you can quantify and certify with confidence.

What Malvern Panalytical’s NMC CRMs provide

Each CRM is prepared from high-purity chemicals, so the whole set carries metrological traceability and ISO 17034 compliance. They span the concentration ranges that matter for real NMC materials, and they arrive ready to use:

• Covering Ni, Mn, and Co, and selected minor elements across NMC-relevant ranges
• Also suitable for NCA, LCO, LMO, and their precursor materials
• Supplied with a fusion recipe and XRF method template
• Usable to prepare secondary pressed-pellet standards

How we used these CRMs and the Revontium EDXRF spectrometer to analyze NMC cathodes and precursors

We put these CRMs to the test on our Revontium EDXRF spectrometer.

• We used a 50 W, 5 mA, 60 kV Ag-anode X-ray tube and four simultaneous high-resolution silicon drift detectors.
• Analysis was performed under vacuum with an oil-free dry pump – no helium required.
• Calibration standards and the validation sample were prepared as 32-mm fused beads by lithium-borate fusion (1:10 sample-to-flux, 1100°C on an Eagon 2 automatic fusion machine).
• We then performed a complete cold-to-cold cycle of approximately 30 minutes.
• Each bead was measured in 4.5 minutes (roughly 13 samples an hour).
• Calibration curves for NiO, CoO, MnO, and SO₃ tracked the certified concentrations closely.

To validate the full method, we ran ten replicate beads of BAM-S014, a certified Li-NMC 111 cathode material. Measured averages sat close to the certified values. When the method was repeated across three days, the differences stayed well within the limits set by ISO Guide 35: evidence that the whole workflow, bead-making included, is both repeatable and stable.

Our advice: Pair NMC-specific CRMs with reproducible fusion and rapid XRF

Accurate, quantitative NMC analysis comes down to three things working together: NMC-specific CRMs to calibrate against, reproducible fused-bead preparation, and fast XRF measurement. Together, these parameters give battery R&D, process control, and quality control teams a robust, efficient route to results – with a 4.5-minute measurement time and a throughput of approximately 13 samples an hour.

Download our application note for the full method and validation data behind our Revontium EDXRF analysis of NMC cathodes and precursors.